Dispersions comprising functionalized oxidic nanoparticles
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example 1
Preparation of ZnO
[0110]73.6 g of zinc acetate dihydrate were suspended in a 421 flask in 2236 ml of 2-propanol and heated to 75° C. In parallel to this, 32.8 g of potassium hydroxide were dissolved in 1168 ml of 2-propanol at 75° C. The KOH solution was then added to the zinc acetate suspension with vigorous stirring, the resulting mixture was heated at 75° C. for 1 hour with stirring and cooled to room temperature. The resulting white precipitate was deposited, the supernatant was filtered off with suction, the white residue was washed with 1000 ml of 2-propanol and deposited. The supernatant was again filtered off with suction, the white residue was again washed with 2-propanol and deposited. After refiltering the liquid supernatant with suction, the white residue was topped up with 2-propanol.
example 2
Functionalization according to the invention of ZnO with 2-[methoxy(polyethyleneoxy)-propyl]trimethoxysilane and subsequent coating with an SiO2-containing layer by hydrolysis of tetramethoxysilane
[0111]Analogously to example 1, 1348 g of a 4.45% by weight dispersion of an unfunctionalized ZnO in 2-propanol were prepared. A solution of 15 g of 2-[methoxy(polyethyleneoxy)propyl]trimethoxysilane in 631 g of 2-propanol was then added dropwise to this solution over the course of 190 minutes with vigorous stirring. The suspension was heated to 60° C. and the mixture was heated under reflux for 30 minutes. 81 g of a 25% strength by weight aqueous NH3 solution were then added and the resulting suspension was heated at 60° C. for 12 hours with stirring. The suspension became transparent during this. Furthermore, a solution of 7.5 g of tetramethoxysilane (TMOS) in 118 g of 2-propanol was added to the resulting suspension over the course of 40 minutes with stirring. The resulting suspension w...
example 3
Dispersion comprising 2-[methoxy(polyethyleneoxy)propyl]trimethoxysilane-functionalized then SiO2-coated ZnO in a polyesterpolyol
[0112]The white residue of functionalized and coated particles FM obtained according to example 2 was redispersed in THF to form a 5% strength by weight ZnO dispersion. The average particle size determined by means of DLS was 25 nm (% by volume). TEM analysis confirmed the amorphous Si-containing coating around ZnO particles. In total, ca. 1150 g of a 5% by weight ZnO dispersion in THF were prepared.
[0113]Furthermore, a solution comprising 1000 g of a difunctional polyesterpolyol and 1000 g of THF was prepared. The polyesterpolyol had a molecular weight of 2000 and was prepared from adipic acid and equimolar amounts of 1,4-butanediol and ethylene glycol. 1150 g of the aforementioned redispersed ZnO dispersion in THF were added to this solution. The resulting mixture remained transparent.
[0114]The composition obtained corresponds to ca. 2.3 parts by weight ...
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Abstract
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